#------------------------------------------------------------------------------ #$Date: 2020-02-25 04:07:18 +0200 (Tue, 25 Feb 2020) $ #$Revision: 248427 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557374.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557374 loop_ _publ_author_name 'Xu, Niansheng' 'Zheng, Aibin' 'Wei, Yuefang' 'Yuan, Yi' 'Zhang, Jing' 'Lei, Ming' 'Wang, Peng' _publ_section_title ; D-\p-D molecular semiconductors for perovskite solar cells: the superior role of helical versus planar \p-linker ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC00362J _journal_year 2020 _chemical_formula_moiety '2(C48 H38 N2 O4 S), C H2 Cl2' _chemical_formula_sum 'C97 H78 Cl2 N4 O8 S2' _chemical_formula_weight 1562.65 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-12-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-08-24 deposited with the CCDC. 2020-02-24 downloaded from the CCDC. ; _cell_angle_alpha 85.956(5) _cell_angle_beta 83.941(5) _cell_angle_gamma 82.064(5) _cell_formula_units_Z 1 _cell_length_a 10.5796(14) _cell_length_b 13.7266(18) _cell_length_c 14.3680(18) _cell_measurement_reflns_used 6615 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 32.65 _cell_measurement_theta_min 2.30 _cell_volume 2051.7(5) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 170.01 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_unetI/netI 0.1016 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 35678 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.270 _diffrn_reflns_theta_min 2.301 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1560 before and 0.0755 after correction. The Ratio of minimum to maximum transmission is 0.8997. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.265 _exptl_crystal_description needle _exptl_crystal_F_000 818 _exptl_crystal_size_max 0.521 _exptl_crystal_size_mid 0.073 _exptl_crystal_size_min 0.065 _refine_diff_density_max 2.583 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 527 _refine_ls_number_reflns 15578 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.1839 _refine_ls_R_factor_gt 0.1059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3102 _refine_ls_wR_factor_ref 0.3784 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7712 _reflns_number_total 15578 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc00362j2.cif _cod_data_source_block 181207_dnt1_0m _cod_database_code 1557374 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.988 _shelx_estimated_absorpt_t_min 0.907 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: C49(0.5) H49A(0.5) H49B(0.5) Cl1(0.5) Cl2(0.5) 3.a Secondary CH2 refined with riding coordinates: C49(H49A,H49B) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33), C36(H36), C37(H37), C39(H39), C40(H40), C43(H43), C44(H44), C46(H46), C47(H47) 3.c Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C48(H48A,H48B, H48C) ; _shelx_res_file ; TITL 181207_dnt1_0m_a.res in P-1 181207_dnt1_0m.res created by SHELXL-2016/6 at 11:38:23 on 11-Dec-2018 REM Old TITL 181207_DNT1_0m in P-1 REM SHELXT solution in P-1 REM R1 0.194, Rweak 0.010, Alpha 0.050, Orientation as input REM Formula found by SHELXT: C48 N7 O S CELL 0.71073 10.5796 13.7266 14.368 85.956 83.941 82.064 ZERR 1 0.0014 0.0018 0.0018 0.005 0.005 0.005 LATT 1 SFAC C H Cl N O S UNIT 97 78 2 4 8 2 L.S. 10 0 0 PLAN 20 SIZE 0.065 0.073 0.521 TEMP -103.14 BOND $H htab list 4 fmap 2 53 acta OMIT -1 -1 1 OMIT -1 0 1 REM REM REM WGHT 0.200000 FVAR 0.60148 S1 6 0.222199 0.399658 0.741357 11.00000 0.02833 0.04829 = 0.03063 -0.00935 0.00489 -0.00884 O1 5 -0.270230 0.006324 0.784413 11.00000 0.04528 0.04807 = 0.03656 0.00715 0.00356 -0.01471 O2 5 -0.133417 0.352511 0.158616 11.00000 0.04805 0.08025 = 0.03122 0.00803 -0.01023 -0.02119 O3 5 0.486060 0.864781 0.958994 11.00000 0.08040 0.04114 = 0.07765 -0.02466 0.02485 -0.00780 O4 5 1.064093 0.238785 0.935356 11.00000 0.05029 0.04852 = 0.06349 -0.00719 -0.02710 0.00358 N1 4 0.021576 0.207560 0.507886 11.00000 0.02439 0.04478 = 0.03812 0.00518 -0.00751 -0.01412 N2 4 0.659136 0.501480 0.805821 11.00000 0.03642 0.03637 = 0.03759 -0.01221 -0.01291 -0.00221 C1 1 0.116707 0.297575 0.614783 11.00000 0.02013 0.03873 = 0.03686 -0.00253 0.00130 -0.00690 AFIX 43 H1 2 0.034919 0.313020 0.648398 11.00000 -1.20000 AFIX 0 C2 1 0.130585 0.241253 0.538917 11.00000 0.02118 0.03906 = 0.03382 0.00085 -0.00546 -0.01100 C3 1 0.256948 0.207758 0.494964 11.00000 0.02861 0.03379 = 0.02846 -0.00263 -0.00377 -0.00821 C4 1 0.275311 0.133532 0.430310 11.00000 0.03029 0.04134 = 0.03742 -0.00770 -0.00767 -0.01107 AFIX 43 H4 2 0.202846 0.111656 0.408598 11.00000 -1.20000 AFIX 0 C5 1 0.396533 0.092106 0.398012 11.00000 0.03906 0.04014 = 0.04460 -0.01509 -0.00475 -0.00586 AFIX 43 H5 2 0.407140 0.042271 0.354144 11.00000 -1.20000 AFIX 0 C6 1 0.503857 0.123134 0.429550 11.00000 0.03070 0.03559 = 0.04507 -0.01161 -0.00277 -0.00228 AFIX 43 H6 2 0.587274 0.092709 0.408782 11.00000 -1.20000 AFIX 0 C7 1 0.489516 0.197328 0.490372 11.00000 0.02226 0.03596 = 0.03635 -0.00824 -0.00242 -0.00361 AFIX 43 H7 2 0.563708 0.217643 0.510964 11.00000 -1.20000 AFIX 0 C8 1 0.366355 0.244732 0.523487 11.00000 0.02318 0.03230 = 0.02814 -0.00178 -0.00457 -0.00461 C9 1 0.347088 0.317126 0.592985 11.00000 0.02281 0.03144 = 0.02644 -0.00180 -0.00342 -0.00421 C10 1 0.225446 0.332608 0.642695 11.00000 0.02324 0.03687 = 0.02932 -0.00467 0.00053 -0.00466 C11 1 0.383606 0.411648 0.715336 11.00000 0.02753 0.03652 = 0.02662 -0.00399 -0.00165 -0.00621 C12 1 0.436183 0.371432 0.631415 11.00000 0.02242 0.03016 = 0.02528 -0.00403 -0.00272 -0.00434 C13 1 0.560066 0.397507 0.593019 11.00000 0.02405 0.02299 = 0.02500 -0.00304 -0.00330 0.00004 C14 1 0.605196 0.392635 0.496638 11.00000 0.02470 0.02739 = 0.02601 -0.00196 -0.00332 -0.00201 AFIX 43 H14 2 0.554322 0.368753 0.454842 11.00000 -1.20000 AFIX 0 C15 1 0.721245 0.421891 0.462801 11.00000 0.02929 0.03463 = 0.03170 0.00073 0.00166 -0.00063 AFIX 43 H15 2 0.749971 0.417704 0.398116 11.00000 -1.20000 AFIX 0 C16 1 0.797099 0.457683 0.522804 11.00000 0.02918 0.03550 = 0.04162 -0.00190 0.00100 -0.01036 AFIX 43 H16 2 0.878781 0.475137 0.499279 11.00000 -1.20000 AFIX 0 C17 1 0.754621 0.467856 0.615493 11.00000 0.02881 0.03281 = 0.03777 -0.00547 -0.00364 -0.00908 AFIX 43 H17 2 0.806892 0.492757 0.655629 11.00000 -1.20000 AFIX 0 C18 1 0.633393 0.441568 0.652057 11.00000 0.02580 0.02749 = 0.03029 -0.00252 -0.00620 -0.00449 C19 1 0.580702 0.465469 0.744863 11.00000 0.02981 0.03401 = 0.02734 -0.00697 -0.00494 -0.00488 C20 1 0.454819 0.457290 0.773302 11.00000 0.03568 0.03901 = 0.02654 -0.00871 -0.00147 -0.00802 AFIX 43 H20 2 0.416034 0.481943 0.831127 11.00000 -1.20000 AFIX 0 C21 1 -0.054809 0.154857 0.576379 11.00000 0.02475 0.03171 = 0.03251 0.00079 -0.00400 -0.00844 C22 1 0.001978 0.069018 0.621166 11.00000 0.02625 0.04063 = 0.04807 0.00218 -0.00314 -0.00218 AFIX 43 H22 2 0.088904 0.044829 0.602789 11.00000 -1.20000 AFIX 0 C23 1 -0.065522 0.018567 0.691576 11.00000 0.03411 0.03540 = 0.04494 0.00273 -0.00518 -0.00153 AFIX 43 H23 2 -0.024334 -0.038510 0.722808 11.00000 -1.20000 AFIX 0 C24 1 -0.194148 0.051394 0.716843 11.00000 0.03423 0.03175 = 0.03272 -0.00463 -0.00258 -0.01232 C25 1 -0.253077 0.135898 0.670759 11.00000 0.02708 0.03554 = 0.03845 -0.00558 -0.00077 -0.00337 AFIX 43 H25 2 -0.341417 0.157933 0.686361 11.00000 -1.20000 AFIX 0 C26 1 -0.182688 0.187454 0.602393 11.00000 0.02905 0.03233 = 0.03716 0.00242 -0.00560 -0.00418 AFIX 43 H26 2 -0.222620 0.246092 0.572833 11.00000 -1.20000 AFIX 0 C27 1 -0.211432 -0.078253 0.834417 11.00000 0.05624 0.06476 = 0.06269 0.02583 -0.00181 -0.01567 AFIX 137 H27A 2 -0.178250 -0.129382 0.790566 11.00000 -1.50000 H27B 2 -0.274909 -0.103287 0.881419 11.00000 -1.50000 H27C 2 -0.140676 -0.060290 0.865674 11.00000 -1.50000 AFIX 0 C28 1 -0.020105 0.241615 0.420062 11.00000 0.02344 0.03526 = 0.03296 0.00091 -0.00336 -0.00628 C29 1 -0.114036 0.201487 0.381117 11.00000 0.02986 0.03365 = 0.03549 -0.00195 -0.00593 -0.01030 AFIX 43 H29 2 -0.151393 0.148642 0.414499 11.00000 -1.20000 AFIX 0 C30 1 -0.155574 0.236152 0.294455 11.00000 0.02920 0.04341 = 0.03558 -0.00672 -0.00678 -0.00767 AFIX 43 H30 2 -0.221401 0.207915 0.270124 11.00000 -1.20000 AFIX 0 C31 1 -0.100137 0.312423 0.243628 11.00000 0.03209 0.05353 = 0.02819 -0.00342 -0.00162 -0.00447 C32 1 -0.004991 0.351923 0.281631 11.00000 0.03380 0.05102 = 0.03319 0.00477 -0.00088 -0.01578 AFIX 43 H32 2 0.034589 0.402898 0.246816 11.00000 -1.20000 AFIX 0 C33 1 0.034292 0.319797 0.368302 11.00000 0.02796 0.04276 = 0.03613 0.00263 -0.00303 -0.01133 AFIX 43 H33 2 0.097812 0.350090 0.393284 11.00000 -1.20000 AFIX 0 C34 1 -0.234276 0.314939 0.120553 11.00000 0.04218 0.08571 = 0.03710 0.00372 -0.01150 -0.01166 AFIX 137 H34A 2 -0.243399 0.344570 0.057137 11.00000 -1.50000 H34B 2 -0.314618 0.331088 0.160250 11.00000 -1.50000 H34C 2 -0.214381 0.243243 0.118016 11.00000 -1.50000 AFIX 0 C35 1 0.612383 0.593156 0.847848 11.00000 0.02827 0.03706 = 0.03512 -0.01107 -0.00531 -0.00667 C36 1 0.584531 0.597220 0.944099 11.00000 0.03295 0.04053 = 0.03327 -0.00478 -0.00086 -0.01099 AFIX 43 H36 2 0.596433 0.538655 0.983299 11.00000 -1.20000 AFIX 0 C37 1 0.539092 0.686931 0.983688 11.00000 0.03445 0.05177 = 0.03680 -0.01537 0.00539 -0.01384 AFIX 43 H37 2 0.518785 0.689107 1.049575 11.00000 -1.20000 AFIX 0 C38 1 0.523731 0.771975 0.927520 11.00000 0.03784 0.03556 = 0.05793 -0.01456 0.01077 -0.00917 C39 1 0.549301 0.767425 0.829902 11.00000 0.04941 0.03725 = 0.05331 0.00209 0.00647 -0.00571 AFIX 43 H39 2 0.535006 0.825533 0.790379 11.00000 -1.20000 AFIX 0 C40 1 0.594880 0.679182 0.791606 11.00000 0.04415 0.04333 = 0.03641 -0.00588 -0.00062 -0.00918 AFIX 43 H40 2 0.614706 0.677008 0.725677 11.00000 -1.20000 AFIX 0 C41 1 0.449196 0.871954 1.058196 11.00000 0.12199 0.07385 = 0.08830 -0.05425 0.04135 -0.02032 AFIX 137 H41A 2 0.429615 0.941487 1.072524 11.00000 -1.50000 H41B 2 0.519790 0.840413 1.093384 11.00000 -1.50000 H41C 2 0.373164 0.838828 1.076004 11.00000 -1.50000 AFIX 0 C42 1 0.761113 0.436336 0.840769 11.00000 0.03026 0.03482 = 0.02743 -0.00275 -0.00376 -0.00592 C43 1 0.773745 0.335407 0.827861 11.00000 0.03826 0.03641 = 0.04082 -0.00551 -0.01300 -0.00970 AFIX 43 H43 2 0.711534 0.309861 0.796840 11.00000 -1.20000 AFIX 0 C44 1 0.875407 0.272297 0.859577 11.00000 0.04526 0.03305 = 0.04473 -0.00675 -0.01107 -0.00735 AFIX 43 H44 2 0.882759 0.204008 0.849468 11.00000 -1.20000 AFIX 0 C45 1 0.966954 0.307263 0.906003 11.00000 0.03550 0.04084 = 0.03639 -0.00415 -0.00655 -0.00566 C46 1 0.956166 0.407463 0.918944 11.00000 0.02926 0.04310 = 0.03301 -0.00807 -0.00461 -0.00751 AFIX 43 H46 2 1.018658 0.432608 0.950009 11.00000 -1.20000 AFIX 0 C47 1 0.853820 0.471299 0.886454 11.00000 0.02984 0.03640 = 0.03115 -0.00604 -0.00223 -0.00973 AFIX 43 H47 2 0.847344 0.539731 0.895679 11.00000 -1.20000 AFIX 0 C48 1 1.151999 0.272575 0.988898 11.00000 0.04807 0.06283 = 0.06053 0.00315 -0.02917 -0.00510 AFIX 137 H48A 2 1.195369 0.323095 0.951740 11.00000 -1.50000 H48B 2 1.215656 0.217321 1.006470 11.00000 -1.50000 H48C 2 1.106004 0.300770 1.045658 11.00000 -1.50000 AFIX 0 C49 1 0.209945 0.093620 0.799636 10.50000 0.07224 0.05708 = 0.07847 -0.02623 -0.02981 0.01528 AFIX 23 H49A 2 0.136820 0.112375 0.761472 10.50000 -1.20000 H49B 2 0.220336 0.151816 0.833674 10.50000 -1.20000 AFIX 0 PART 1 CL1 3 0.171210 -0.007026 0.886283 10.50000 0.15965 0.09246 = 0.12487 -0.02468 -0.04041 0.03467 CL2 3 0.341568 0.064665 0.728526 10.50000 0.10880 0.17993 = 0.08282 -0.03951 0.00716 0.08478 HKLF 4 REM 181207_dnt1_0m_a.res in P-1 REM R1 = 0.1059 for 7712 Fo > 4sig(Fo) and 0.1839 for all 15578 data REM 527 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y+1, -z+2 HTAB C41 O1_$1 EQIV $2 x-1, y, z HTAB C49 O4_$2 REM Highest difference peak 2.583, deepest hole -0.455, 1-sigma level 0.125 Q1 1 0.2947 -0.0023 0.7634 11.00000 0.05 2.58 Q2 1 0.1285 -0.0514 0.9333 11.00000 0.05 1.68 Q3 1 0.3956 0.1251 0.7647 11.00000 0.05 1.57 Q4 1 0.2256 0.0165 0.8982 11.00000 0.05 1.57 Q5 1 0.2002 -0.0242 0.8394 11.00000 0.05 1.51 Q6 1 0.3239 0.0802 0.7129 11.00000 0.05 1.42 Q7 1 0.1495 0.0111 0.8833 11.00000 0.05 0.99 Q8 1 0.2766 0.0567 0.8451 11.00000 0.05 0.66 Q9 1 0.4403 0.2035 0.5118 11.00000 0.05 0.35 Q10 1 0.9857 0.3563 0.8969 11.00000 0.05 0.35 Q11 1 0.3392 0.1002 0.4356 11.00000 0.05 0.34 Q12 1 0.4445 0.1423 0.4052 11.00000 0.05 0.33 Q13 1 0.0033 0.3698 0.2868 11.00000 0.05 0.33 Q14 1 0.4965 0.3875 0.6167 11.00000 0.05 0.32 Q15 1 0.8957 0.4393 0.8970 11.00000 0.05 0.31 Q16 1 0.5601 0.6234 0.8155 11.00000 0.05 0.31 Q17 1 0.9171 0.4226 0.8801 11.00000 0.05 0.30 Q18 1 0.0164 0.2958 0.3841 11.00000 0.05 0.30 Q19 1 0.3562 0.2256 0.6821 11.00000 0.05 0.30 Q20 1 0.8186 0.4604 0.8395 11.00000 0.05 0.29 ; _shelx_res_checksum 9045 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.22220(8) 0.39966(7) 0.74136(5) 0.0356(2) Uani 1 1 d . . . . . O1 O -0.2702(2) 0.00632(19) 0.78441(17) 0.0435(6) Uani 1 1 d . . . . . O2 O -0.1334(3) 0.3525(2) 0.15862(17) 0.0520(7) Uani 1 1 d . . . . . O3 O 0.4861(3) 0.8648(2) 0.9590(3) 0.0677(10) Uani 1 1 d . . . . . O4 O 1.0641(3) 0.2388(2) 0.9354(2) 0.0533(7) Uani 1 1 d . . . . . N1 N 0.0216(2) 0.2076(2) 0.50789(19) 0.0349(6) Uani 1 1 d . . . . . N2 N 0.6591(3) 0.5015(2) 0.80582(19) 0.0359(6) Uani 1 1 d . . . . . C1 C 0.1167(3) 0.2976(2) 0.6148(2) 0.0319(6) Uani 1 1 d . . . . . H1 H 0.034919 0.313020 0.648398 0.038 Uiso 1 1 calc R . . . . C2 C 0.1306(3) 0.2413(2) 0.5389(2) 0.0306(6) Uani 1 1 d . . . . . C3 C 0.2569(3) 0.2078(2) 0.4950(2) 0.0298(6) Uani 1 1 d . . . . . C4 C 0.2753(3) 0.1335(3) 0.4303(2) 0.0352(7) Uani 1 1 d . . . . . H4 H 0.202846 0.111656 0.408598 0.042 Uiso 1 1 calc R . . . . C5 C 0.3965(3) 0.0921(3) 0.3980(3) 0.0405(7) Uani 1 1 d . . . . . H5 H 0.407140 0.042271 0.354144 0.049 Uiso 1 1 calc R . . . . C6 C 0.5039(3) 0.1231(2) 0.4295(2) 0.0369(7) Uani 1 1 d . . . . . H6 H 0.587274 0.092709 0.408782 0.044 Uiso 1 1 calc R . . . . C7 C 0.4895(3) 0.1973(2) 0.4904(2) 0.0313(6) Uani 1 1 d . . . . . H7 H 0.563708 0.217643 0.510964 0.038 Uiso 1 1 calc R . . . . C8 C 0.3664(3) 0.2447(2) 0.5235(2) 0.0276(6) Uani 1 1 d . . . . . C9 C 0.3471(3) 0.3171(2) 0.59298(19) 0.0268(5) Uani 1 1 d . . . . . C10 C 0.2254(3) 0.3326(2) 0.6427(2) 0.0298(6) Uani 1 1 d . . . . . C11 C 0.3836(3) 0.4116(2) 0.7153(2) 0.0300(6) Uani 1 1 d . . . . . C12 C 0.4362(3) 0.3714(2) 0.63142(19) 0.0257(5) Uani 1 1 d . . . . . C13 C 0.5601(3) 0.3975(2) 0.59302(19) 0.0242(5) Uani 1 1 d . . . . . C14 C 0.6052(3) 0.3926(2) 0.49664(19) 0.0261(5) Uani 1 1 d . . . . . H14 H 0.554322 0.368753 0.454842 0.031 Uiso 1 1 calc R . . . . C15 C 0.7212(3) 0.4219(2) 0.4628(2) 0.0327(6) Uani 1 1 d . . . . . H15 H 0.749971 0.417704 0.398116 0.039 Uiso 1 1 calc R . . . . C16 C 0.7971(3) 0.4577(2) 0.5228(2) 0.0352(7) Uani 1 1 d . . . . . H16 H 0.878781 0.475137 0.499279 0.042 Uiso 1 1 calc R . . . . C17 C 0.7546(3) 0.4679(2) 0.6155(2) 0.0325(6) Uani 1 1 d . . . . . H17 H 0.806892 0.492757 0.655629 0.039 Uiso 1 1 calc R . . . . C18 C 0.6334(3) 0.4416(2) 0.6521(2) 0.0275(6) Uani 1 1 d . . . . . C19 C 0.5807(3) 0.4655(2) 0.7449(2) 0.0299(6) Uani 1 1 d . . . . . C20 C 0.4548(3) 0.4573(2) 0.7733(2) 0.0332(6) Uani 1 1 d . . . . . H20 H 0.416034 0.481943 0.831127 0.040 Uiso 1 1 calc R . . . . C21 C -0.0548(3) 0.1549(2) 0.5764(2) 0.0292(6) Uani 1 1 d . . . . . C22 C 0.0020(3) 0.0690(3) 0.6212(3) 0.0388(7) Uani 1 1 d . . . . . H22 H 0.088904 0.044829 0.602789 0.047 Uiso 1 1 calc R . . . . C23 C -0.0655(3) 0.0186(3) 0.6916(3) 0.0386(7) Uani 1 1 d . . . . . H23 H -0.024334 -0.038510 0.722808 0.046 Uiso 1 1 calc R . . . . C24 C -0.1941(3) 0.0514(2) 0.7168(2) 0.0321(6) Uani 1 1 d . . . . . C25 C -0.2531(3) 0.1359(2) 0.6708(2) 0.0338(6) Uani 1 1 d . . . . . H25 H -0.341417 0.157933 0.686361 0.041 Uiso 1 1 calc R . . . . C26 C -0.1827(3) 0.1875(2) 0.6024(2) 0.0329(6) Uani 1 1 d . . . . . H26 H -0.222620 0.246092 0.572833 0.039 Uiso 1 1 calc R . . . . C27 C -0.2114(5) -0.0783(4) 0.8344(3) 0.0622(12) Uani 1 1 d . . . . . H27A H -0.178250 -0.129382 0.790566 0.093 Uiso 1 1 calc GR . . . . H27B H -0.274909 -0.103287 0.881419 0.093 Uiso 1 1 calc GR . . . . H27C H -0.140676 -0.060290 0.865674 0.093 Uiso 1 1 calc GR . . . . C28 C -0.0201(3) 0.2416(2) 0.4201(2) 0.0304(6) Uani 1 1 d . . . . . C29 C -0.1140(3) 0.2015(2) 0.3811(2) 0.0322(6) Uani 1 1 d . . . . . H29 H -0.151393 0.148642 0.414499 0.039 Uiso 1 1 calc R . . . . C30 C -0.1556(3) 0.2362(3) 0.2945(2) 0.0353(7) Uani 1 1 d . . . . . H30 H -0.221401 0.207915 0.270124 0.042 Uiso 1 1 calc R . . . . C31 C -0.1001(3) 0.3124(3) 0.2436(2) 0.0381(7) Uani 1 1 d . . . . . C32 C -0.0050(3) 0.3519(3) 0.2816(2) 0.0389(7) Uani 1 1 d . . . . . H32 H 0.034589 0.402898 0.246816 0.047 Uiso 1 1 calc R . . . . C33 C 0.0343(3) 0.3198(3) 0.3683(2) 0.0352(7) Uani 1 1 d . . . . . H33 H 0.097812 0.350090 0.393284 0.042 Uiso 1 1 calc R . . . . C34 C -0.2343(4) 0.3149(4) 0.1206(3) 0.0545(11) Uani 1 1 d . . . . . H34A H -0.243399 0.344570 0.057137 0.082 Uiso 1 1 calc GR . . . . H34B H -0.314618 0.331088 0.160250 0.082 Uiso 1 1 calc GR . . . . H34C H -0.214381 0.243243 0.118016 0.082 Uiso 1 1 calc GR . . . . C35 C 0.6124(3) 0.5932(2) 0.8478(2) 0.0327(6) Uani 1 1 d . . . . . C36 C 0.5845(3) 0.5972(3) 0.9441(2) 0.0350(7) Uani 1 1 d . . . . . H36 H 0.596433 0.538655 0.983299 0.042 Uiso 1 1 calc R . . . . C37 C 0.5391(3) 0.6869(3) 0.9837(3) 0.0403(8) Uani 1 1 d . . . . . H37 H 0.518785 0.689107 1.049575 0.048 Uiso 1 1 calc R . . . . C38 C 0.5237(4) 0.7720(3) 0.9275(3) 0.0439(8) Uani 1 1 d . . . . . C39 C 0.5493(4) 0.7674(3) 0.8299(3) 0.0477(9) Uani 1 1 d . . . . . H39 H 0.535006 0.825533 0.790379 0.057 Uiso 1 1 calc R . . . . C40 C 0.5949(4) 0.6792(3) 0.7916(3) 0.0410(8) Uani 1 1 d . . . . . H40 H 0.614706 0.677008 0.725677 0.049 Uiso 1 1 calc R . . . . C41 C 0.4492(7) 0.8720(4) 1.0582(4) 0.095(2) Uani 1 1 d . . . . . H41A H 0.429615 0.941487 1.072524 0.143 Uiso 1 1 calc GR . . . . H41B H 0.519790 0.840413 1.093384 0.143 Uiso 1 1 calc GR . . . . H41C H 0.373164 0.838828 1.076004 0.143 Uiso 1 1 calc GR . . . . C42 C 0.7611(3) 0.4363(2) 0.8408(2) 0.0306(6) Uani 1 1 d . . . . . C43 C 0.7737(3) 0.3354(2) 0.8279(2) 0.0372(7) Uani 1 1 d . . . . . H43 H 0.711534 0.309861 0.796840 0.045 Uiso 1 1 calc R . . . . C44 C 0.8754(4) 0.2723(3) 0.8596(3) 0.0401(7) Uani 1 1 d . . . . . H44 H 0.882759 0.204008 0.849468 0.048 Uiso 1 1 calc R . . . . C45 C 0.9670(3) 0.3073(3) 0.9060(2) 0.0372(7) Uani 1 1 d . . . . . C46 C 0.9562(3) 0.4075(3) 0.9189(2) 0.0345(7) Uani 1 1 d . . . . . H46 H 1.018658 0.432608 0.950009 0.041 Uiso 1 1 calc R . . . . C47 C 0.8538(3) 0.4713(2) 0.8865(2) 0.0318(6) Uani 1 1 d . . . . . H47 H 0.847344 0.539731 0.895679 0.038 Uiso 1 1 calc R . . . . C48 C 1.1520(4) 0.2726(3) 0.9889(3) 0.0559(11) Uani 1 1 d . . . . . H48A H 1.195369 0.323095 0.951740 0.084 Uiso 1 1 calc GR . . . . H48B H 1.215656 0.217321 1.006470 0.084 Uiso 1 1 calc GR . . . . H48C H 1.106004 0.300770 1.045658 0.084 Uiso 1 1 calc GR . . . . C49 C 0.2099(10) 0.0936(7) 0.7996(7) 0.069(3) Uani 0.5 1 d . . P . . H49A H 0.136820 0.112375 0.761472 0.083 Uiso 0.5 1 calc R . P A . H49B H 0.220336 0.151816 0.833674 0.083 Uiso 0.5 1 calc R . P A . Cl1 Cl 0.1712(5) -0.0070(3) 0.8863(3) 0.1277(15) Uani 0.5 1 d . . P B 1 Cl2 Cl 0.3416(4) 0.0647(4) 0.7285(3) 0.1333(18) Uani 0.5 1 d . . P B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0283(4) 0.0483(5) 0.0306(4) -0.0093(3) 0.0049(3) -0.0088(3) O1 0.0453(14) 0.0481(15) 0.0366(12) 0.0071(11) 0.0036(10) -0.0147(11) O2 0.0480(16) 0.080(2) 0.0312(12) 0.0080(13) -0.0102(10) -0.0212(14) O3 0.080(2) 0.0411(16) 0.078(2) -0.0247(15) 0.0249(18) -0.0078(15) O4 0.0503(16) 0.0485(16) 0.0635(17) -0.0072(13) -0.0271(13) 0.0036(12) N1 0.0244(12) 0.0448(16) 0.0381(13) 0.0052(12) -0.0075(10) -0.0141(10) N2 0.0364(14) 0.0364(14) 0.0376(14) -0.0122(11) -0.0129(11) -0.0022(11) C1 0.0201(13) 0.0387(16) 0.0369(15) -0.0025(13) 0.0013(11) -0.0069(11) C2 0.0212(13) 0.0391(16) 0.0338(14) 0.0009(12) -0.0055(10) -0.0110(11) C3 0.0286(14) 0.0338(15) 0.0285(13) -0.0026(12) -0.0038(11) -0.0082(11) C4 0.0303(15) 0.0413(18) 0.0374(16) -0.0077(13) -0.0077(12) -0.0111(12) C5 0.0391(18) 0.0401(18) 0.0446(18) -0.0151(15) -0.0047(14) -0.0059(14) C6 0.0307(15) 0.0356(17) 0.0451(18) -0.0116(14) -0.0028(13) -0.0023(12) C7 0.0223(13) 0.0360(16) 0.0364(15) -0.0082(13) -0.0024(11) -0.0036(11) C8 0.0232(13) 0.0323(15) 0.0281(13) -0.0018(11) -0.0046(10) -0.0046(10) C9 0.0228(13) 0.0314(14) 0.0264(12) -0.0018(11) -0.0034(10) -0.0042(10) C10 0.0232(13) 0.0369(16) 0.0293(13) -0.0047(12) 0.0005(10) -0.0047(11) C11 0.0275(14) 0.0365(16) 0.0266(13) -0.0040(12) -0.0017(10) -0.0062(11) C12 0.0224(12) 0.0302(14) 0.0253(12) -0.0040(11) -0.0027(9) -0.0043(10) C13 0.0241(12) 0.0230(12) 0.0250(12) -0.0030(10) -0.0033(9) 0.0000(9) C14 0.0247(13) 0.0274(14) 0.0260(12) -0.0020(11) -0.0033(10) -0.0020(10) C15 0.0293(15) 0.0346(16) 0.0317(14) 0.0007(12) 0.0017(11) -0.0006(11) C16 0.0292(15) 0.0355(16) 0.0416(17) -0.0019(13) 0.0010(12) -0.0104(12) C17 0.0288(14) 0.0328(15) 0.0378(15) -0.0055(13) -0.0036(12) -0.0091(11) C18 0.0258(13) 0.0275(14) 0.0303(13) -0.0025(11) -0.0062(10) -0.0045(10) C19 0.0298(14) 0.0340(15) 0.0273(13) -0.0070(12) -0.0049(11) -0.0049(11) C20 0.0357(16) 0.0390(17) 0.0265(13) -0.0087(12) -0.0015(11) -0.0080(12) C21 0.0248(13) 0.0317(14) 0.0325(14) 0.0008(12) -0.0040(11) -0.0084(11) C22 0.0263(15) 0.0406(18) 0.0481(19) 0.0022(15) -0.0031(13) -0.0022(12) C23 0.0341(17) 0.0354(17) 0.0449(18) 0.0027(14) -0.0052(13) -0.0015(13) C24 0.0342(16) 0.0317(15) 0.0327(14) -0.0046(12) -0.0026(12) -0.0123(12) C25 0.0271(14) 0.0355(16) 0.0385(16) -0.0056(13) -0.0008(12) -0.0034(11) C26 0.0291(15) 0.0323(15) 0.0372(15) 0.0024(13) -0.0056(12) -0.0042(11) C27 0.056(3) 0.065(3) 0.063(3) 0.026(2) -0.002(2) -0.016(2) C28 0.0234(13) 0.0353(15) 0.0330(14) 0.0009(12) -0.0034(11) -0.0063(11) C29 0.0299(15) 0.0336(15) 0.0355(15) -0.0019(12) -0.0059(12) -0.0103(12) C30 0.0292(15) 0.0434(18) 0.0356(15) -0.0067(14) -0.0068(12) -0.0077(12) C31 0.0321(16) 0.054(2) 0.0282(14) -0.0034(14) -0.0016(12) -0.0045(14) C32 0.0338(17) 0.051(2) 0.0332(15) 0.0048(15) -0.0009(12) -0.0158(14) C33 0.0280(15) 0.0428(18) 0.0361(15) 0.0026(14) -0.0030(12) -0.0113(12) C34 0.042(2) 0.086(3) 0.0371(18) 0.0037(19) -0.0115(15) -0.0117(19) C35 0.0283(14) 0.0371(16) 0.0351(15) -0.0111(13) -0.0053(11) -0.0067(12) C36 0.0329(16) 0.0405(17) 0.0333(15) -0.0048(13) -0.0009(12) -0.0110(13) C37 0.0345(17) 0.052(2) 0.0368(16) -0.0154(15) 0.0054(13) -0.0138(14) C38 0.0378(18) 0.0356(18) 0.058(2) -0.0146(16) 0.0108(16) -0.0092(14) C39 0.049(2) 0.0373(19) 0.053(2) 0.0021(16) 0.0065(17) -0.0057(15) C40 0.0442(19) 0.0433(19) 0.0364(16) -0.0059(15) -0.0006(14) -0.0092(15) C41 0.122(5) 0.074(4) 0.088(4) -0.054(3) 0.041(4) -0.020(3) C42 0.0303(14) 0.0348(16) 0.0274(13) -0.0028(12) -0.0038(11) -0.0059(11) C43 0.0383(17) 0.0364(17) 0.0408(17) -0.0055(14) -0.0130(13) -0.0097(13) C44 0.045(2) 0.0331(16) 0.0447(18) -0.0067(14) -0.0111(15) -0.0074(14) C45 0.0355(17) 0.0408(18) 0.0364(16) -0.0041(14) -0.0066(13) -0.0057(13) C46 0.0293(15) 0.0431(18) 0.0330(15) -0.0081(13) -0.0046(12) -0.0075(12) C47 0.0298(15) 0.0364(16) 0.0311(14) -0.0060(12) -0.0022(11) -0.0097(12) C48 0.048(2) 0.063(3) 0.061(2) 0.003(2) -0.0292(19) -0.0051(18) C49 0.072(6) 0.057(5) 0.078(6) -0.026(5) -0.030(5) 0.015(4) Cl1 0.160(4) 0.092(3) 0.125(3) -0.025(2) -0.040(3) 0.035(2) Cl2 0.109(3) 0.180(4) 0.083(2) -0.040(2) 0.0072(19) 0.085(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S1 C10 90.53(14) . . ? C24 O1 C27 117.0(3) . . ? C31 O2 C34 117.2(3) . . ? C38 O3 C41 117.1(4) . . ? C45 O4 C48 116.9(3) . . ? C2 N1 C21 116.4(2) . . ? C28 N1 C2 120.2(2) . . ? C28 N1 C21 122.3(2) . . ? C19 N2 C35 117.9(3) . . ? C42 N2 C19 118.8(3) . . ? C42 N2 C35 121.4(2) . . ? C2 C1 H1 120.4 . . ? C2 C1 C10 119.1(3) . . ? C10 C1 H1 120.4 . . ? N1 C2 C3 119.4(3) . . ? C1 C2 N1 120.1(3) . . ? C1 C2 C3 120.3(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 C8 119.4(3) . . ? C8 C3 C2 119.5(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H4 119.5 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.1(3) . . ? C6 C5 H5 119.9 . . ? C5 C6 H6 119.9 . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.9 . . ? C6 C7 H7 119.1 . . ? C6 C7 C8 121.7(3) . . ? C8 C7 H7 119.1 . . ? C3 C8 C9 119.0(3) . . ? C7 C8 C3 117.2(3) . . ? C7 C8 C9 123.2(3) . . ? C8 C9 C12 131.6(3) . . ? C10 C9 C8 117.1(3) . . ? C10 C9 C12 110.8(3) . . ? C1 C10 S1 123.7(2) . . ? C9 C10 S1 113.2(2) . . ? C9 C10 C1 123.1(3) . . ? C12 C11 S1 113.2(2) . . ? C12 C11 C20 123.1(3) . . ? C20 C11 S1 123.6(2) . . ? C11 C12 C9 111.5(2) . . ? C11 C12 C13 117.0(3) . . ? C13 C12 C9 131.2(3) . . ? C14 C13 C12 123.2(2) . . ? C14 C13 C18 117.9(3) . . ? C18 C13 C12 118.5(2) . . ? C13 C14 H14 119.5 . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.5 . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.4(3) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 119.8 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 119.7 . . ? C16 C17 C18 120.6(3) . . ? C18 C17 H17 119.7 . . ? C13 C18 C19 120.1(3) . . ? C17 C18 C13 119.2(3) . . ? C17 C18 C19 120.6(3) . . ? N2 C19 C18 119.3(3) . . ? C20 C19 N2 120.4(3) . . ? C20 C19 C18 120.2(3) . . ? C11 C20 H20 120.5 . . ? C19 C20 C11 118.9(3) . . ? C19 C20 H20 120.5 . . ? C22 C21 N1 119.0(3) . . ? C26 C21 N1 122.5(3) . . ? C26 C21 C22 118.5(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 C21 121.3(3) . . ? C23 C22 H22 119.4 . . ? C22 C23 H23 120.1 . . ? C22 C23 C24 119.9(3) . . ? C24 C23 H23 120.1 . . ? O1 C24 C23 124.7(3) . . ? O1 C24 C25 115.9(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25 120.0 . . ? C21 C26 H26 119.5 . . ? C25 C26 C21 121.0(3) . . ? C25 C26 H26 119.5 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 C33 120.0(3) . . ? C29 C28 N1 122.4(3) . . ? C29 C28 C33 117.6(3) . . ? C28 C29 H29 118.9 . . ? C28 C29 C30 122.1(3) . . ? C30 C29 H29 118.9 . . ? C29 C30 H30 120.1 . . ? C29 C30 C31 119.8(3) . . ? C31 C30 H30 120.1 . . ? O2 C31 C30 124.9(3) . . ? O2 C31 C32 116.7(3) . . ? C32 C31 C30 118.4(3) . . ? C31 C32 H32 118.9 . . ? C33 C32 C31 122.2(3) . . ? C33 C32 H32 118.9 . . ? C28 C33 H33 120.0 . . ? C32 C33 C28 119.9(3) . . ? C32 C33 H33 120.0 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N2 121.1(3) . . ? C40 C35 N2 119.7(3) . . ? C40 C35 C36 119.2(3) . . ? C35 C36 H36 119.8 . . ? C35 C36 C37 120.3(3) . . ? C37 C36 H36 119.8 . . ? C36 C37 H37 120.0 . . ? C38 C37 C36 120.1(3) . . ? C38 C37 H37 120.0 . . ? O3 C38 C39 115.4(4) . . ? C37 C38 O3 125.1(4) . . ? C37 C38 C39 119.5(3) . . ? C38 C39 H39 120.0 . . ? C40 C39 C38 120.0(4) . . ? C40 C39 H39 120.0 . . ? C35 C40 H40 119.6 . . ? C39 C40 C35 120.8(3) . . ? C39 C40 H40 119.6 . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 N2 120.9(3) . . ? C47 C42 N2 120.9(3) . . ? C47 C42 C43 118.1(3) . . ? C42 C43 H43 119.6 . . ? C44 C43 C42 120.9(3) . . ? C44 C43 H43 119.6 . . ? C43 C44 H44 119.6 . . ? C43 C44 C45 120.9(3) . . ? C45 C44 H44 119.6 . . ? O4 C45 C44 116.6(3) . . ? O4 C45 C46 124.4(3) . . ? C44 C45 C46 118.9(3) . . ? C45 C46 H46 119.9 . . ? C45 C46 C47 120.2(3) . . ? C47 C46 H46 119.9 . . ? C42 C47 C46 121.0(3) . . ? C42 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? O4 C48 H48A 109.5 . . ? O4 C48 H48B 109.5 . . ? O4 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? H49A C49 H49B 107.7 . . ? Cl1 C49 H49A 108.8 . . ? Cl1 C49 H49B 108.8 . . ? Cl2 C49 H49A 108.8 . . ? Cl2 C49 H49B 108.8 . . ? Cl2 C49 Cl1 113.9(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C10 1.739(3) . ? S1 C11 1.737(3) . ? O1 C24 1.364(4) . ? O1 C27 1.424(5) . ? O2 C31 1.364(4) . ? O2 C34 1.421(5) . ? O3 C38 1.374(4) . ? O3 C41 1.444(7) . ? O4 C45 1.373(4) . ? O4 C48 1.412(5) . ? N1 C2 1.424(4) . ? N1 C21 1.428(4) . ? N1 C28 1.408(4) . ? N2 C19 1.424(4) . ? N2 C35 1.437(4) . ? N2 C42 1.414(4) . ? C1 H1 0.9500 . ? C1 C2 1.364(5) . ? C1 C10 1.412(4) . ? C2 C3 1.446(4) . ? C3 C4 1.407(4) . ? C3 C8 1.434(4) . ? C4 H4 0.9500 . ? C4 C5 1.376(5) . ? C5 H5 0.9500 . ? C5 C6 1.395(5) . ? C6 H6 0.9500 . ? C6 C7 1.371(4) . ? C7 H7 0.9500 . ? C7 C8 1.423(4) . ? C8 C9 1.438(4) . ? C9 C10 1.401(4) . ? C9 C12 1.453(4) . ? C11 C12 1.391(4) . ? C11 C20 1.411(4) . ? C12 C13 1.449(4) . ? C13 C14 1.419(4) . ? C13 C18 1.424(4) . ? C14 H14 0.9500 . ? C14 C15 1.374(4) . ? C15 H15 0.9500 . ? C15 C16 1.394(5) . ? C16 H16 0.9500 . ? C16 C17 1.370(5) . ? C17 H17 0.9500 . ? C17 C18 1.418(4) . ? C18 C19 1.432(4) . ? C19 C20 1.369(4) . ? C20 H20 0.9500 . ? C21 C22 1.394(4) . ? C21 C26 1.386(4) . ? C22 H22 0.9500 . ? C22 C23 1.378(5) . ? C23 H23 0.9500 . ? C23 C24 1.391(5) . ? C24 C25 1.397(4) . ? C25 H25 0.9500 . ? C25 C26 1.383(4) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.384(4) . ? C28 C33 1.415(4) . ? C29 H29 0.9500 . ? C29 C30 1.394(4) . ? C30 H30 0.9500 . ? C30 C31 1.395(5) . ? C31 C32 1.383(5) . ? C32 H32 0.9500 . ? C32 C33 1.378(4) . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.387(4) . ? C35 C40 1.385(5) . ? C36 H36 0.9500 . ? C36 C37 1.396(5) . ? C37 H37 0.9500 . ? C37 C38 1.372(6) . ? C38 C39 1.404(6) . ? C39 H39 0.9500 . ? C39 C40 1.371(5) . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.397(5) . ? C42 C47 1.390(4) . ? C43 H43 0.9500 . ? C43 C44 1.380(5) . ? C44 H44 0.9500 . ? C44 C45 1.387(5) . ? C45 C46 1.388(5) . ? C46 H46 0.9500 . ? C46 C47 1.395(4) . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C49 Cl1 1.853(12) . ? C49 Cl2 1.657(11) . ?